CN104409683B - A kind of method preparing anode and cathode lithium ion battery side by side based on coaxial 3D printing technique - Google Patents
A kind of method preparing anode and cathode lithium ion battery side by side based on coaxial 3D printing technique Download PDFInfo
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- CN104409683B CN104409683B CN201410238059.4A CN201410238059A CN104409683B CN 104409683 B CN104409683 B CN 104409683B CN 201410238059 A CN201410238059 A CN 201410238059A CN 104409683 B CN104409683 B CN 104409683B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/106—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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Abstract
The present invention relates to a kind of method preparing anode and cathode lithium ion battery side by side based on coaxial 3D printing technique.This method is mainly first prepared and is comprised lithium titanate, Kynoar, the anode of LiFePO4 mixture, barrier film and negative electrode marking ink respectively, by 3D printing technique, use the anode and cathode side by side configuration that coaxial sleeve 3D printing technique prints with lithium titanate as anode material, Kynoar is as diaphragm material, LiFePO4 is as cathode material, this anode and cathode side by side configuration have anode, barrier film coaxial and with negative electrode special construction side by side, finally transfer to glove box is packaged by this structure, obtain coaxial anode and cathode lithium ion battery side by side further.The method is mainly printing last layer porous septum outside anode material, and can be in close contact with cathode material, substantially reduce lithium ion diffusion length between anodic-cathodic, improve the electrical conductivity of electrode material, have huge application potential in high performance lithium ion battery field.
Description
Technical field
The invention belongs to 3D technology and the combination of new forms of energy nm regime, relate generally to a kind of method preparing anode and cathode lithium ion battery side by side based on coaxial 3D printing technique.
Background technology
Along with the exhaustion day by day of traditional energy, lithium rechargeable battery represents thus of great interest as new forms of energy.Lithium ion battery is as the main power source of mobile communication equipment Yu mancarried electronic aid simultaneously, has the advantages such as higher, without memory, the high-energy-density of output voltage due to it and becomes the focus of research both at home and abroad.But generally there is the problems such as specific surface area is the highest, energy storage density is limited, electrode polarization is serious in tradition lithium ion battery based on plane electrode.
Recently as nanometer technology and the rise of 3D printing technique, nanometer technology and 3D printing technique have been extended to military affairs, electronics, medical science, biological, the fields such as new forms of energy, the most novel 3D prints the appearance of integrated lithium ion battery, effectively achieve the effective integration of lithium ion battery anode and cathode and package system thereof, revolutionize conventional planar electrode type lithium ion battery structure, this will substantially increase the ratio of active material in battery electrode material, shorten the migration distance in lithium ion charge and discharge process, thus substantially increase lithium ion diffusion rate and mobility.
But, existing typically use aseptate anode and cathode interdigital structure based on the lithium ion battery prepared by 3D printing technique, although this structure is easily achieved 3D and prints, but due to lithium ion battery electrode material, in lithium storing process, Volume Changes is notable and stress is bigger, this interdigital structure electrode is easily deformable in its charge and discharge process even to cave in, cause anode and cathode short circuit, open circuit or formation to electrocute block, ultimately cause that cycle performance is deteriorated, the decay of lithium memory capacity is fast.
Summary of the invention
For shortcomings and deficiencies of the prior art, the invention provides a kind of method preparing anode and cathode lithium ion battery side by side based on coaxial 3D printing technique.This method is mainly dissolved in respective solution prepares each printing electrode ink with lithium titanate, polyimides, LiFePO4 respectively, recycling 3D printing technique, prepare with lithium titanate as anode material, polyimides is barrier film, LiFePO4 be the anode barrier film of cathode material coaxial and with negative electrode special construction side by side.Electrode material prepared by the method has the advantages such as specific surface area is big, energy density is high, anode and cathode electrode spacing is little.These all will greatly improve lithium ion diffusion velocity in-between the electrodes, and then improve its ion and electronic conductivity, simultaneously, coaxial due to anode barrier film and with negative electrode special construction side by side existence makes the Stability Analysis of Structures of battery, therefore, there is huge application potential in high performance lithium ion battery field.
Technical solution of the present invention is as follows:
A kind of method preparing anode and cathode lithium ion battery side by side based on coaxial 3D printing technique, it is characterized in that: utilize 3D printing technique to prepare with lithium titanate as anode material, with porous polyvinylidene fluoride film as barrier film, with LiFePO4 for cathode material anode and cathode li-ion electrode side by side, prepare anode and cathode lithium ion battery side by side by encapsulation the most again.
Wherein, described preparation method comprises the following steps:
1) weigh ultrasonic the dissolving in 100-150ml deionized waters and 60-80ml glycerine of 3-5g LiFePO4 and form the first mixed solution；Weigh that 5-10g lithium titanate is ultrasonic to be dissolved in the second mixed solution being made up of 3-5g polymethyl methacrylate, 100-200ml deionized water and 60-80ml glycerine, weigh 3-5g Kynoar and dissolve in the 3rd mixed solution that 60-100ml is made up of 1-METHYLPYRROLIDONE, polyethylene glycol, LiCl, polymethyl methacrylate；
2) by after above-mentioned three kinds of mixed solutions ball milling 24-48h respectively, transfer in centrifuge, filter after processing 5-10min under 3500-4500rpm and remove large particulate matter, transfer to filtrate respectively the most again centrifuge filters after centrifugal treating 3-5h under 3000-4000rpm；
3) three kinds of materials of gained after above-mentioned filtration are distributed in the mixed solution being made up of glycerine, hydroxypropyl cellulose, hydroxyethyl cellulose and deionized water respectively, strong stirring 1-3h；
4) take sheet glass that specification is 20 × 10mm as substrate, utilize mask plate to hide evaporation coating techniques and prepare graphical gold electrode at glass substrate surface, respectively as cell cathode and anode current collector；
5) the 3D printer with coaxial sleeve printhead is utilized to print with lithium titanate as anode material, with Kynoar as diaphragm material at substrate surface, and utilize common micro-spray printhead to print iron lithium phosphate cathode material, the most respectively negative electrode, anode material are printed to cell cathode and anode current collector region；
6) glass substrate of printed side-by-side electrode material is placed in tube furnace at 100-300 DEG C heating 3-5 hour；
7) after utilizing poly methyl methacrylate plastic plate and dimethyl silicone polymer fluid sealant coaxial electrode material surrounding to be impaled along glass substrate; transfer in glove box; electrolyte is instilled under argon shield; to cover above it with poly methyl methacrylate plastic plate and dimethyl silicone polymer fluid sealant and seal again after complete wetting, i.e. obtain forming the coaxial lithium ion battery of anode and cathode.
Described coaxial sleeve printhead includes inside and outside two-layer, respectively its mixed solution rate of extrusion of programme-control.
The dissolving 1-METHYLPYRROLIDONE of Kynoar, polyethylene glycol, LiCl, the mass fraction of four kinds of materials of polymethyl methacrylate are respectively 75%, 10%, 5% and 10%.
In mixed solution described in step 3), glycerine, hydroxypropyl cellulose, hydroxyethyl cellulose and deionized water, the mass fraction of four kinds of materials is respectively 50%, 15%, 5% and 30%.
The structure of electrode is: Kynoar porous septum is coated on outside lithium titanate anode material, and this structure then directly and membrane contacts, is repeated i.e. can to obtain the electrode structure of this anode and cathode lithium ion battery side by side by lithiated-iron-phosphate cathode the most again.
Advantages of the present invention is: prepare with LiFePO4 as cathode material, and with porous polyvinylidene fluoride film as barrier film, the coaxial side by side configuration with lithium titanate as anode material, this preparation method has the advantage that technique is simply accurate, controllability is high.Prepared electrode material specific surface area is big, can be effectively improved material electric conductivity, be the development inexorable trend of new type lithium ion battery preparation technology.
Accompanying drawing explanation
Fig. 1 is the Structure of the cathode and the anode schematic diagram side by side that 3D printing technique prints
Fig. 2 is electrode structure (the including encapsulation) schematic diagram of the final lithium ion battery that 3D printing technique prints
Detailed description of the invention
It is desirable to provide a kind of method preparing anode and cathode lithium ion battery side by side based on coaxial 3D printing technique, illustrate in conjunction with accompanying drawing and specific embodiment
Embodiment 1
1) weigh in the 3g LiFePO4 ultrasonic 100ml of dissolving in deionized water and 60ml glycerine and form the first mixed solution；Weigh that 5g lithium titanate is ultrasonic to be dissolved in the second mixed solution being made up of 3g PMMA (polymethyl methacrylate), 100ml deionized water and 60ml glycerine.Weigh 3g Kynoar to dissolve in the 3rd mixed solution that 60ml is made up of 1-METHYLPYRROLIDONE, polyethylene glycol, LiCl, PMMA.
2) by after above-mentioned three kinds of mixed solutions ball milling 24h respectively, transfer in centrifuge, filter after processing 5min under 3500rpm and remove large particulate matter, transfer to filtrate respectively the most again centrifuge filters after centrifugal treating 3h under 3000rpm.
3) three kinds of materials of gained after above-mentioned filtration are distributed to respectively by glycerine, HPC(hydroxypropyl cellulose), HEC(hydroxyethyl cellulose) and the mixed solution that forms of deionized water in, strong stirring 1h.
4) take sheet glass that specification is 20 × 10mm as substrate, utilize mask plate to hide evaporation coating techniques and prepare graphical gold electrode at glass substrate surface, respectively as cell cathode and anode current collector；
5) utilize the 3D printer with coaxial sleeve printhead to print with lithium titanate as anode material, with Kynoar as diaphragm material at substrate surface, and utilize common micro-spray printhead to print iron lithium phosphate cathode material.The most respectively negative electrode, anode material are printed to cell cathode and anode current collector region.Fig. 1 is side-by-side electrode chip architecture schematic diagram, wherein 1 represents porous septum, and 2 represent anode, and 3 represent negative electrode.
6) glass substrate of printed side-by-side electrode material is placed in tube furnace 100oHeat 3-5 hour under C.
7) after utilizing PMMA (polymethyl methacrylate) plastic plate and PDMS (dimethyl silicone polymer) fluid sealant coaxial electrode material surrounding to be impaled along glass substrate; transfer in glove box; electrolyte is instilled under argon shield; to cover above it with PMMA plastic plate and PDMS fluid sealant and seal again after complete wetting, i.e. obtain forming the coaxial lithium ion battery of anode and cathode.Fig. 2 is the coaxial lithium ion battery of anode and cathode side by side after encapsulation, wherein 4 represents glass substrate, and 5 represent cathode collector.
Embodiment 2
1) weigh in the 4g LiFePO4 ultrasonic 120ml of dissolving in deionized water and 70ml glycerine and form the first mixed solution；Weigh that 7g lithium titanate is ultrasonic to be dissolved in the second mixed solution being made up of 4g PMMA (polymethyl methacrylate), 150ml deionized water and 70ml glycerine.Weigh 4g Kynoar to dissolve in the 3rd mixed solution that 80ml is made up of 1-METHYLPYRROLIDONE, polyethylene glycol, LiCl, PMMA.
2) by after above-mentioned three kinds of mixed solutions ball milling 36h respectively, transfer in centrifuge, filter after processing 7min under 4000rpm and remove large particulate matter, transfer to filtrate respectively the most again centrifuge filters after centrifugal treating 4h under 3500rpm.
3) three kinds of materials of gained after above-mentioned filtration are distributed to respectively by glycerine, HPC(hydroxypropyl cellulose), HEC(hydroxyethyl cellulose) and the mixed solution that forms of deionized water in, strong stirring 2h.
4) take sheet glass that specification is 20 × 10mm as substrate, utilize mask plate to hide evaporation coating techniques and prepare graphical gold electrode at glass substrate surface, respectively as cell cathode and anode current collector；
5) utilize the 3D printer with coaxial sleeve printhead to print with lithium titanate as anode material, with Kynoar as diaphragm material at substrate surface, and utilize common micro-spray printhead to print iron lithium phosphate cathode material.The most respectively negative electrode, anode material are printed to cell cathode and anode current collector region.Fig. 1 is side-by-side electrode chip architecture schematic diagram, wherein 1 represents porous septum, and 2 represent anode, and 3 represent negative electrode.
6) glass substrate of printed side-by-side electrode material is placed in tube furnace 200oHeat 4 hours under C.
7) after utilizing PMMA (polymethyl methacrylate) plastic plate and PDMS (dimethyl silicone polymer) fluid sealant coaxial electrode material surrounding to be impaled along glass substrate; transfer in glove box; electrolyte is instilled under argon shield; to cover above it with PMMA plastic plate and PDMS fluid sealant and seal again after complete wetting, i.e. obtain forming the coaxial lithium ion battery of anode and cathode.Fig. 2 is the coaxial lithium ion battery of anode and cathode side by side after encapsulation, wherein 4 represents glass substrate, and 5 represent cathode collector.
Embodiment 3
1) weigh in the 5g LiFePO4 ultrasonic 150ml of dissolving in deionized water and 80ml glycerine and form the first mixed solution；Weigh that 10g lithium titanate is ultrasonic to be dissolved in the second mixed solution being made up of 5g PMMA (polymethyl methacrylate), 200ml deionized water and 80ml glycerine.Weigh 5g Kynoar to dissolve in the 3rd mixed solution that 100ml is made up of 1-METHYLPYRROLIDONE, polyethylene glycol, LiCl, PMMA.
2) by after above-mentioned three kinds of mixed solutions ball milling 48h respectively, transfer in centrifuge, filter after processing 10min under 4500rpm and remove large particulate matter, transfer to filtrate respectively the most again centrifuge filters after centrifugal treating 5h under 4000rpm.
3) three kinds of materials of gained after above-mentioned filtration are distributed to respectively by glycerine, HPC(hydroxypropyl cellulose), HEC(hydroxyethyl cellulose) and the mixed solution that forms of deionized water in, strong stirring 3h.
4) take sheet glass that specification is 20 × 10mm as substrate, utilize mask plate to hide evaporation coating techniques and prepare graphical gold electrode at glass substrate surface, respectively as cell cathode and anode current collector；
5) utilize the 3D printer with coaxial sleeve printhead to print with lithium titanate as anode material, with Kynoar as diaphragm material at substrate surface, and utilize common micro-spray printhead to print iron lithium phosphate cathode material.The most respectively negative electrode, anode material are printed to cell cathode and anode current collector region.Fig. 1 is side-by-side electrode chip architecture schematic diagram, wherein 1 represents porous septum, and 2 represent anode, and 3 represent negative electrode.
6) glass substrate of printed side-by-side electrode material is placed in tube furnace 300oHeat 5 hours under C.
7) after utilizing PMMA (polymethyl methacrylate) plastic plate and PDMS (dimethyl silicone polymer) fluid sealant coaxial electrode material surrounding to be impaled along glass substrate; transfer in glove box; electrolyte is instilled under argon shield; to cover above it with PMMA plastic plate and PDMS fluid sealant and seal again after complete wetting, i.e. obtain forming the coaxial lithium ion battery of anode and cathode.Fig. 2 is the coaxial lithium ion battery of anode and cathode side by side after encapsulation, wherein 4 represents glass substrate, and 5 represent cathode collector.
Claims (5)
1. the method preparing anode and cathode lithium ion battery side by side based on coaxial 3D printing technique, it is characterised in that: comprise the following steps:
1) weigh ultrasonic the dissolving in 100-150ml deionized waters and 60-80ml glycerine of 3-5g LiFePO4 and form the first mixed solution；Weigh that 5-10g lithium titanate is ultrasonic to be dissolved in the second mixed solution being made up of 3-5g polymethyl methacrylate, 100-200ml deionized water and 60-80ml glycerine, weigh 3-5g Kynoar and dissolve in the 3rd mixed solution that 60-100ml is made up of 1-METHYLPYRROLIDONE, polyethylene glycol, LiCl, polymethyl methacrylate；
2) by after above-mentioned three kinds of mixed solutions ball milling 24-48h respectively, transfer in centrifuge, filter after processing 5-10min under 3500-4500rpm and remove large particulate matter, transfer to filtrate respectively the most again centrifuge filters after centrifugal treating 3-5h under 3000-4000rpm；
3) three kinds of materials of gained after above-mentioned filtration are distributed in the mixed solution being made up of glycerine, hydroxypropyl cellulose, hydroxyethyl cellulose and deionized water respectively, strong stirring 1-3h；
4) take sheet glass that specification is 20 × 10mm as substrate, utilize mask plate to hide evaporation coating techniques and prepare graphical gold electrode at glass substrate surface, respectively as cell cathode and anode current collector；
5) the 3D printer with coaxial sleeve printhead is utilized to print with lithium titanate as anode material, with Kynoar as diaphragm material at substrate surface, and utilize common micro-spray printhead to print iron lithium phosphate cathode material, the most respectively negative electrode, anode material are printed to cell cathode and anode current collector region；
6) glass substrate of printed side-by-side electrode material is placed in tube furnace at 100-300oHeat 3-5 hour under C；
7) after utilizing poly methyl methacrylate plastic plate and dimethyl silicone polymer fluid sealant coaxial electrode material surrounding to be impaled along glass substrate; transfer in glove box; electrolyte is instilled under argon shield; to cover above it with poly methyl methacrylate plastic plate and dimethyl silicone polymer fluid sealant and seal again after complete wetting, i.e. obtain forming the coaxial lithium ion battery of anode and cathode.
A kind of method preparing anode and cathode lithium ion battery side by side based on coaxial 3D printing technique the most according to claim 1, it is characterised in that: the coaxial sleeve printhead described in step 5) includes inside and outside two-layer, respectively its mixed solution rate of extrusion of programme-control.
A kind of method preparing anode and cathode lithium ion battery side by side based on coaxial 3D printing technique the most according to claim 2, it is characterised in that: the dissolving 1-METHYLPYRROLIDONE of Kynoar, polyethylene glycol, LiCl, the mass fraction of four kinds of materials of polymethyl methacrylate are respectively 75%, 10%, 5% and 10%.
A kind of method preparing anode and cathode lithium ion battery side by side based on coaxial 3D printing technique the most according to claim 2, it is characterized in that: in the mixed solution described in step 3), glycerine, hydroxypropyl cellulose, hydroxyethyl cellulose and deionized water, the mass fraction of four kinds of materials is respectively 50%, 15%, 5% and 30%.
A kind of method preparing anode and cathode lithium ion battery side by side based on coaxial 3D printing technique the most according to claim 2, it is characterized in that: the structure of electrode is: Kynoar porous septum is coated on outside lithium titanate anode material, this structure then directly and membrane contacts, is repeated i.e. can to obtain the electrode structure of this anode and cathode lithium ion battery side by side by lithiated-iron-phosphate cathode the most again.
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| EP3121875A1 (en) | 2015-07-20 | 2017-01-25 | Centre National De La Recherche Scientifique | Method for manufacturing a miniaturized electrochemical cell and a miniaturized electrochemical cell |
| CN108110314B (en) * | 2017-12-18 | 2021-01-22 | 惠州亿纬创能电池有限公司 | Battery module and method for manufacturing same |
| CN112549526A (en) * | 2019-09-10 | 2021-03-26 | 北京大学 | Printing head with multilayer core-shell structure and method for printing micro device by adopting printing head |
| CN112164595A (en) * | 2020-09-27 | 2021-01-01 | 福州大学 | Multi-core-shell coaxial structure functional device and preparation method thereof |
| CN115703632B (en) * | 2021-08-11 | 2023-11-28 | 中天新兴材料有限公司 | Polyimide recovery processing method |
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